Finishing cellulosic textile fabric



United States Patent 9 ce FINISHING CELLULOSIC TEXTILE FABRIC William B. Canter, Danville, Va,, assignor to Dan River Mills, Incorporated, Danville, Va.

No Drawing. Application May 9, 1955 Serial No. 507,173

Claims. (21. 117-65) The present invention relates to the treatment of textile fabrics to produce wrinkle resistance and to attain a permanent full soft hand which cannot be produced by prior methods.

It is an object of this invention to obtain a permanent exceptionally full but still soft hand. Another object of the invention is the incorporation of wrinkle resistance and dimensional stability with the desired hand. Still a third object of the invention is the simplification of the procedural steps for obtaining desired hands on starch sized cotton fabrics as they are treated to obtain wrinkle resistance. Other objects of the invention will be obvious from the following specification.

The objects of this invention are obtained by the process which generally comprises impregnating textile fabrics woven from warps sized with starch and starch products, with thermosetting resin forming materials, catalyst, and amylase (starch converting enzymes) at the same time; storing the impregnated fabrics under conditions favorable to enzyme activity for a period of time long enough to hydrolyze the starch partially, to a point short of sugar; and heating the fabric to effect drying, to halt the enzyme activity, to cure the resin and to fix the partially hydrolyzed starch products in a washfast condition on the fabric. The amount of enzyme used must be regulated to compensate for any adverse effect caused by the resin and catalyst. Preferably, the storage period is from about 1 to 4 hours at a temperature of from about 140 F. to 180 F. It is also preferable to use an amine hydrochloride as the catalyst.

Fabrics treated in accordance with this process are characterized by the usual properties of wrinkle resistance expected from the thermosetting resin forming material used, but by a hand which is fuller than can be obtained by prior art methods without sacrificing softness. These fabrics are further characterized by good dimensional stability and permanence of the desired properties of hand, wrinkle resistance and dimensional stability even after laundering. It should be noted that the resistance to the laundering is a function of the resin chosen and varies from resin to resin, as would be expected.

The present invention is particularly directed to the processing of fabrics which have been woven from warps sized with starch. Many modifications of starch and many starch formulas are commonly used in the textile industry for sizing cellulosic textiles, and especially for sizing cotton warps. tion can be satisfactorily used on fabrics having warps sized with any of these various formulas. The nature of the amylase used in the process of this invention does not appear to be critical in that the invention has been used with equal success on several of the commercially available enzymes recommended for desizing starch. Generally, these enzymes are the bacterial type, and they are sold under the trade names of Rapidase, Ergase, Excise, etc.

It has been found that a wide variety of water soluble, thermosetting resin-forming materials may be used inthe It appears that the present inven-' 2,808,341 l atented Oct. 1, 1957 process of this invention. Among the resin-forming materials which have been tested and found satisfactory are: dimethylolurea, dimethyl ether of trimethylol melamine, dimethylolethylene urea, a condensation product of urea, acrolein and formaldehyde, and 1,3-dimethy1ol, S-ethyl tetrahydro-Z, (1)-s-triazone. It appears that one may successfully use any resin-forming material useful for obtaining wrinkle resistance on cellulosic fabrics.

However, it has been found that both resin-forming materials, loosely called resins, and catalysts have some adverse effect on the amylase activity, and some care should be exercised in the choice and use of these materials. Inasmuch as commercial enzymes have a rather wide range of activity from container to container and from time to time, most textile" desizing operationsemploy an excess of enzyme more than adequate to offset any effect of a resin used in accordance with this invention.

Generally speaking, all resins heretofore used in treat ing textiles for wrinkle resistance appear to be useful in the process of the present invention, as the adverse effect of the resin is, in most instances, adequately overcome by the excess of enzymes.

Catalysts must be chosen and used with more care, as some, such as zinc nitrate, will kill more than 50% of the effectiveness of ordinary enzymes. This does not mean that such catalysts are inoperative in the process of the present invention, but that an additional amount of enzyme should be added, or that the period of enzyme activity must be increased. Most other catalysts have asmaller adverse effect which also may be overcome in a similar manner. Such catalysts are magnesium chlm ride and di-ammonium phosphates. Latent catalysts such as monoethanol amine hydrochloride have only a negligible effect on enzyme activity and such catalysts are the preferred ones for this invention for that reason.

The effect of resin-forming materials and catalysts on enzyme activity can be objectively determined by the procedure of Sink and Worth, as described in The American Dyestutf Reporter at volume 40, page 848, dated December 24, 1951. Using this procedure in a laboratory simulation of the impregnation and storage stepsof the present invention with stock solutions of 5% resin, .5% catalyst, .15% enzyme and 5% starch, all by weight, it was determined that the adverse effect of various resin- Thus, one treating starch sized fabrics in accordance with this invention can use any combination of resin andcatalysts desired, provided the quantity of enzyme is regu lated to offset the adverse effects of the material chosen. It will also be seen that, as a practical matter, the amount of enzyme usually used for desizing combined with any resin used for obtaining wrinkle resistance may be used in the proces of the present invention without altering the usual qualities of such materials, provided an. amine, hydrochloride catalyst is used.

In carrying out the invention, ityi's also enable,

p 2,808,341 p g 3 4 sometimes advantageous, to incorporate other materials, Example V such as wetting agents, softening agents and the like.

The invention will be better understood by reference to the following typical examples:

The process of Example I was repeated using 5 pounds of Rhozyme LA instead of 2.5 pounds and using a tandem arrangement of pad, drying tenter and curing oven without a separate storage step, The fabric produced by the process of this example was satisfactory for drapery material but was not as soft as the fabric of the preceding examples. The large amount of enzyme used was enough to partially hydrolyze the starch in the early stage of drying before the temperature of the fabric became high enough to kill the enzyme acticity.

Example I An all-cotton fabric woven from warps sized with about of their weight of corn starch containing a small portion of wax and softener, was padded with about 70% of its weight of an aqueous liquid from a 40 gallon 10 mix containing:

5 P 0 0f PIOSOteX (@Wetting d Softening agent Thus, it will be seenthat the gist of the present inldellfified as a modified mlxture 0f mmefal and Vegevention is the simultaneous impregnation of starch sized table Oil sulfflllates) cotton fabrics with amylase, resin and catalyst, followed 4 Pounds of Triton X400 lwll'ianic Wetting agent by a period of high temperature storage to effect partial identified as an y 'y p alcohcl) hydrolysis of the starch, and a heating operation to effect P 0f RhOZYmB LA bacterial enzyme idellfidrying and to cure the resin. Fabrics processed fled as a Standardized diastall'c enzyme Preparation in accordance with the invention are characterized by a liquid form) fuller soft hand than can be obtained by prior art 33 pounds of Zeset S (about 50% solids solution of methods dimethylol ethylene urea) 1 l i 6% Pounds of 50% Solution of monoeihanol amine y- 1. The method of treating cotton textile fabrics to dfochlfll'ide obtain wrinkle resistance and a full, pliable hand, which Rfimaillder Water comprises impregnating a woven starch sized cotton fab- The pad solution was kept at 160 F. and the thus imric with an aqueous liquid Containing as an amylase bacterial enzyme, a water-soluble, thcrmosetting resinforming material which is an aminoplast and an amine hydrochloride catalyst, storing the thus impregnated fabric for from about one to four hours at a temperature from about 140 F. to 180 F. to partially hydrolyze the starch and thereafter heating the fabric containing the partially hydrolized starch, aminoplast and catalyst to effect drying and'to cure the aminoplast.

. 2. The method of treating cellulosis textile fabrics to obtain wrinkle resistance and a full, pliable hand, which comprises impregnating a woven starch sized cellulosic fabric with an aqueous liquid containing amylase, a water soluble, thermosetting resin-forming material and a catalyst forpolymeriziug the resin on the fabric, storing the thus impregnated fabric at a temperature from about 140 F. to 180 F. for a time suffiicient to hydrolyze the starch substantially, but short of conversion to sugar, and thereafter heating the fabric containing the partially hydrolized starch, resin and catalyst to effect drying and to cure the resin, said catalyst being one that does not Example H lower the activity of amylase below about 50% of its normal activity on starch at room temperature.

. 3. The method of treating cellulosic textile fabrics to obtain wrinkle resistance and a full pliable hand which comprises impregnating a woven starch sized cellulosic fabric with an aqueous liquid containing amylase, a water soluble thermosetting resin forming material and a catalyst for polymerizing the resin on the fabric, storing the thus impregnated fabric for from about one to four hours at a temperature from about 140 F. to 180 F. and thereafter heating the fabric containing the partially hydrolized starch, resin and catalyst to effect drying and Example In to cure the resin, said catalyst being one that does not lower the activity of amylase below about 50% of its pregnated fabric was batched into rolls at about that temperature. After storing for 4 hours, the fabric was dried on a tenter frame and cured for 70 seconds at 350 F. Part of the fabric was then washed and treated with the water repellent, and another part was sanforized. In each instance, the fabric had good wrinkle resistance and an exceptionally full but soft hand suitable for drapery material. This procedure was repeated several times, varying the storage period from a few seconds to 6 hours. The fabric was progressively softer as the storage time was increased. Below one hour the fabric became appreciably stiffer as the time was decreased, but there was still a noticeable softening effect due to the enzyme even in tandem operation of the pad and tenter frame. As the to storage time was increased beyond 6 hours, white portions of the fabric first became slightly yellow, and then progressively more yellow, indicating that the starch had been converted to sugar, which was carmelized during curing.

The process of Example I was repeated, substituting for the Rhozyme LA (standardized diastatic enzyme preparation in liquid form) other enzymes, namely, Rapidase (standardized mixture containing amlolytic and proteolytic enzymes), Ergase 100 (no specific definition available) and Excise T (standardized solution containing amylolytic and proteolytic enzymes). Each of these enzymes are said by their manufacturers to be of the bacterial type, and each appeared to work in the same manner and with the same effect as the Rhozyme LA.

The process of Example I was repeated, using in place normal activity on Starch at room tempfiratuffi f h Zeset S a condensation product f urea acrolein :4. The method of treating cotton textile fabrics to oband formaldehyde. The results were generally similar to talfl reslsfance and a fun pliable hand which the results obtained in Example I, although hand of the H1555 p g atlng a Woven starch sized cotton fabric fabric of this example was not quite as soft. The differ- Wlth an q us l1qu1 d containmg amylase, a Water soluence in hand may be attributed to the inherent differ ble thermofiljttmg ammoplast RS111 fofmmg mammal and ence in the characteristics of the resin forming materials. 3 'acldlc catalyst for polymerizing the msill 0n the fabric, storing the thus impregnated fabric for from Exa l IV about one to four hours at a temperature from about F. to F. and thereafter heating the fabric con- The process of Example I was repeated, substituting taining the partially hydrolized starch, resin and catalyst for the Zeset the dimethylol ether of trimethylol melato effect drying and to cure the resin, said catalyst being mine. The results were generally the same as those of one that does not lower the activity of amylase below Example 1, except that the processed fabric maintained its about 50% of its normal activity on starch at room hand better on repeated Washing, as is characteristic of temperature.

melamine-treated fabrics. 75 5. The method of treating cellulosic textile fabrics to obtain Wrinkle resistance and a full, pliable hand, which comprises impregnating a woven starch sized cellulosic fabric with an aqueous liquid containing amylase, a water soluble, thermosetting resin-forming material and a catalyst for polymerizing the resin on the fabric, the quantity of amylase being regulated to ofiset adverse effects of the resin and catalyst, storing the thus impregnated fabric for from about one to four hours at a temperature from about 140 F. to 180 F. and thereafter heating the fabric containing the partially hydrolized starch, resin and catalyst to effect drying and to cure the resin, said catalyst being one that does not lower the activity of amylase below about 50% of its normal activity on starch at room temperature.

6. The method of treating cotton textile fabrics to obtain Wrinkle resistance and a full, pliable hand, which comprises impregnating a woven starch sized cotton fabric with an aqueous liquid containing amylase, a watersoluble, thermosetting aminoplast resin-forming material and an acidic catalyst for polymerizing the resin on the fabric, the quantity of amylase being regulated to offset adverse effects of the resin and catalyst, storing the thus impregnated fabric to permit the amylase to partially hydrolyze the starch to a point short of conversion to sugar and thereafter heating the fabric containing the partially hydrolized starch, resin and catalyst to effect drying and to cure the resin, said catalyst being one that does not lower the activity of amylase below about 50% of its normal activity on starch at room temperature.

7. The method of treating cellulosic textile fabrics to obtain wrinkle resistance and a full, pliable hand, which comprises impregnating a woven starch sized cellulosic fabric with an aqueous liquid containing amylase, a watersoluble, thermosetting resin-forming material and a cat alyst for polymerizing the resin on the fabric, the quantity of amylase being regulated to offset any adverse effect of the resin and the catalyst, storing the thus impregnated fabric to permit the amylase to partially hydrolyze the starch to a point short of conversion to sugar and thereafter heating the fabric containing the partially hydrolized starch, resin and catalyst to effect drying and to cure the resin, said catalyst being one that does not lower the activity of amylase below about 50% of its normal activity on starch at room temperature.

8. The method of treating cellulosic textile fabrics to obtain wrinkle resistance and a full, pliable hand which comprises impregnating a woven starch sized cellulosic fabric with an aqueous liquid containing a pancreatic enzyme, a water-soluble, thermosetting resin-forming material and a catalyst for polymerizing the resin on the fabric, storing the thus impregnated fabric for from about one to four hours at a temperature from about 140 F. to 180 F. and thereafter heating the fabric containing the partially hydrolized starch, resin and catalyst to efitect drying and to cure the resin, said catalyst being one that does not lower the activity of amylase below about of its normal activity on starch at room temperature 9. The method of treating celulosic textile fabrics to obtain wrinkle resistance and a full hand which is not boardy which comprises impregnating a woven starch sized cellulosic fabric with an aqueous liquid containing amylase, a water soluble thermosetting resin forming material and an amine hydrochloride catalyst, storing the thus impregnated fabric for from about one to four hours at a temperature from about F. to F. and thereafter heating the fabric containing the partially hydrolized starch, resin and catalyst to effect drying and to cure the resin.

10. The method of treating cellulosic textile fabrics to obtain wrinkle resistance and a full pliable hand which comprises impregnating a woven starch sized cellulosic fabric with an aqueous liquid containing amylase, a water soluble thermosetting resin forming material and a catalyst for polymerizing the resin on the fabric, storing the thus impregnated fabric for a time and at a temperature suflicient to hydrolyze the starch substantially but short of conversion to sugar and thereafter heating the fabric containing the partially hydrolyzed starch, resin and catalyst to effect drying and to cure the resin, said catalyst being one that does not lower the activity of amylase below about 50% of its normal activity on starch at room temperature.

References Cited in the file of this patent UNITED STATES PATENTS 

1.THE METHOD OF TREATING COTTON TEXTILE FABRICS TO OBTAIN WRINKLE RESISTANCE AND A FULL, PLIABLE HAND, WHICH COMPRISES IMPREGNATING A WOVEN STARCH SIZED COTTON FABRIC WITH AN AQUEOUS LIQUID CONTAINING AS AN AMYLASE, A BACTERIAL ENZYME, A WATER-SSOLUBLE, THERMOSETTING RESINFORMING MATERIAL WHICH IS AN AMINOPLAST AND AN AMINE HYDROCHLORIDE CATALYST, STORING THE THUS IMPREGNATED FABRIC FOR FROM ABOUT ONE TO FOUR HOURS AT A TEMPERATURE FROM ABOUT 140*F. TO 180*F. TO PARTIALY HYDROLYZE THE STARCH AND THEREAFTER HEATING THE FABRIC CONTAINING THE PARTIALLY HYDROLIZED STARCH, AMINOPLAST AND CATALYST TO EFFECT DRYING AND TO CURE THE AMINOPLAST. 